Stable suspensions



Patented 14, 1933 umrao srAra-s- PATENT OFFICE osm mam, OI OPPAU, e'nauamr, ASSIGNOB 1'0 I. G, FABBENIRDUSTBE mm- GEELLBCEAFI', OI IBANKIORT-ON 'IHE-HAIN, onnmr s'rannn susrmrsrons Ho Drawing. Application filed March 18, 1981, Serial 150. 623,801, and in Germany larch 89, 1980.

The present invention relates to improvements in the production of stable suspensions, and more particularly of suspensions of materials, capable of forming metal carbonyls, in liquid media.

Suspensions of materials capable of form-' ing metal carbonyls, which term is used here'- in in a broad sense including not only the free metals capable of forming carbonyls or products containing such free metals but also compounds of such metals which can be brought into a form capable of reactingwith carbon monoxide with the formation of metal carbonyls by reduction, as for example the oxides or carbonates of the carbonyl-forming metals, are of particular interest for the manufacture and production of metal carbonyls because recently processes-have been" suggested according to which the said solid initial materials are conve ed into the reaction 'vessel, which is usua y under a rather high pressure, in the form of sus nsions or pastes in suitable liquids such ash uid metal carbonyls or hydrocarbons. Suc

the solid suspended matter tends to settle more or less rapidly and then conveying by meansof pumps or other conve ing devices is of course. rendered difiicult i not impossible at all. Suspensions of the said solid materials in liquid media are of interest also in connection with other fields of the chemi- I have found that very stable suspensions of solids of the nature hereinbefore defined can be prepared b using as the liquid vehicle at least two liquids which are immiscible with each other and which do not dissolve the solid matter to be suspended.

Very good results are obtained in this way for example by the simultaneous em loyment of liquid metal carbonyis on the one and and water or aqueous solutions on the other hand. The material to be suspended may be first made into a paste with the metal carbonyl, the paste then being intimately mixed with a little water which is gradually absorbed by the paste by keeping it in vigorous motion as or example by stirring the mass. The

suspensions, however, often have the drawback that amount of water added will generally range between 1 and 20 per cent by weight of the solid material to be suspended and should preferably be about 10 per cent, whereas the amount of liquid carbonyl should preferably .be about'equal to the weight of the solid matter, though greater or smaller amounts may of course be used. Aqueous solutions of acids, bases, or salts may also be used instead of water without disadvantage though generally the use of water is to be preferred because water does not react with the solid matter to be suspended, as might be the case when adding acids or bases;

- Other combinations 'of at least two liquid media of the aforesaid nature are for example hydrocarbonssuch as gasoline on the one hand and water .or-aqueous solutions on the other hand, or metal carbonyls'or hydrocarbons on the one hand and glycerine or aqueous suspensions of aluminium hydroxide, iron metallic salts are formed in the liquid, filtering the resulting solution and preci itating the hydroxides of the dissolved meta s by the addition of suflicient ammonia, if desired after dilutin the solution. The jelly-like precipitate, i desired after an addition of water, is mixed with a metal carbonyl or a hydroca-bon whereby a stable mixture is obtaine As has been pointed out in the foregoing more than two liquid media of the said nature may be employed, for example very stable pasty masses are obtained by employing water, a metal carbonyl and a hydrocarbon oil ofhigh boiling point as the liquid vehicle.

The size of the solid particles present in the suspensions according tothe present invention should as a rule not exceed 0.25 millimetre in diameter, though in some cases partrate the nature of this invention, butth' ivontionnot restricted to: these examples. I 1

The; parts are'by wsight; I I p iso 'a as of fined grained saw m saa I pyrites which when madeinto a paste alone: I

II with 150: parts of i iron carbonyl rapidly i settled out from the suspension, ara stirred I Withzlfifl parts of iron carbonyl and; 15 parts ofwater. i A paste is formedwhich only step I I aratos a smallamount of carbonyl even when I I allowed to stand for long periods of time and;

' I which may Ibevery satisfactorily-pumped; i I

f I 1:5 parts of aqueous ammonia; solution conprises at leastone materialcapableof torm- I I I ang metal carbonyl and the liquid hase'coms: I I T prises a liquid metal: carbonyl on water. I I I I I As new articles of manufacture stable II prises at least-onemetal napableof forming; I i I metal carbonylv and-the .liquid-phase .co n- I prises at leasttwo liquids, immiscible wlthf each other and not dissolving the solid phase, I 4. new articles of manufacture. stable I I suspensions, of which. the solid? phase com- I prisesat leastonemetalcapableof forming .m etal carbonyl and the liquid phase com-I i I susp'ensions, I of which the solid phase comprises: a liquid metal carbonyl" and. at 'least I f I I, I ione liquid immiscible was I the metal: care I bonyl andnotdissolvingthesolidzyphase. a "gram of hydrogen chlfilidfi P liter, I As :new articlesot manufacture stable I I I I I. vI. iparts,ofcommonsaltsolution containing 100: p ig whi h; the: ii phasg 6mm: i I l l f I I I gr ams'of common 81115991? literymW be prises: at least one metalcapa-bleof forming I I I played ins ead: of the lfipsr s of water wit man carbonyl; and the: {liquid phase; 00111-1 5'3 I i I n fi ST IK w' 'I. :prisesia'liquidzmetal carbonylandwaters ea:4"' V I I Iii-testimony whereof I-haije hereunto set m hand. 'E:fillparts-of isiiclstel;powder-aremadeinto au fl flsKAfifiKfiAlimflkfl i-; 3 :pastewith22Parts'ofironcarhonyh theros f iI:-. sulting. suspension settles very rapidly so 0 z, wuqu; thatalready after4minutestfifl'partsofironz l I i 5 1T mining 1': gram s of ammonia per litezgor .I I I parts of hydrochloric I acid contain-mg 1? .carbonylfreefrom-solid areseparated at the I I top ofthe mixtura After intimatelymixing I I I i with 1,5 parts of .water,; the suspension: is I Z I I I I i I I i very stableand during the said timeonly 9.6 I

.I partof iron-oarbonyl-are separated. I I I o o o o I Similarresults are obtained when prcpari I ingthe paste from parts of nickel powder and 50 parts of iIOIlICfiIbOIlYl and then adding I I 1.5 parts of water.-

Ewamplc 5 100 parts of reduced roasted pyrites are made into a paste with parts of gasolene, whereupon 2 parts of water are added. By intimately mixing the said redients a very stable paste is obtained wh i zh docs not tend to settle even on long standing.

Example 4 1 00 'parts of reduced roasted pyrites are made into a paste with parts oi iron carbonyl. 5 parts of glycerine are added. A stable suspension is obtained. I

Ewample 5 

